CN105784789A - NH3 sensor of mesoporous WO3 material based on supported precious metal Pt and preparation method of NH3 sensor - Google Patents
NH3 sensor of mesoporous WO3 material based on supported precious metal Pt and preparation method of NH3 sensor Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention provides an NH3 sensor of a mesoporous WO3 material based on supported precious metal Pt and a preparation method of the NH3 sensor and belongs to the technical field of semiconductor oxide gas sensors.Precious metal Pt is supported on the mesoporous WO3 material prepared through the hard template method to prepare a sensitive material.By means of the large specific surface area of the mesoporous WO3 material and the catalysis action of Pt on NH3, sensitivity of the sensor to NH3 is effectively improved.Besides, the adopted sensor structure is composed of an Al2O3 insulating ceramic tube with two annular gold electrodes, a semiconductor sensitive material coated on the annular gold electrodes and the Al2O3 insulating ceramic tube, and a nichrome heating coil penetrating through the Al2O3 insulating ceramic tube.The sensor is simple in process, small in size and suitable for large-scale production, and has wide application prospects in the aspect of detection of NH3 content in the microenvironment.
Description
Technical field
The invention belongs to conductor oxidate gas sensor technical field, be specifically related to a kind of based on the mesoporous WO supporting precious metals pt3The NH of material3Gas sensor and preparation method thereof.
Background technology
Ammonia (NH3) may be used for manufacturing ammonia, nitrogenous fertilizer (carbamide, carbon ammonium etc.), compound fertilizer, nitric acid, ammonium salt, soda etc., it is widely used in the fields such as chemical industry, light industry, chemical fertilizer, pharmacy, synthetic fibers.And inorganic salt containing nitrogen and orgnnic comopounds, sulphonamides, polyurethane, Fypro and nitrile rubber etc. all need directly with ammonia for raw material.Additionally, liquefied ammonia is commonly used for cold-producing medium, it is also possible to provide the energy as bio-fuel.Application have universality and popularity.But ammonia has the water solublity of height, is colourless, alkaline irritative gas, eyes and mucosa are had strong impulse.Not only can skin ambustion, eyes, respiratory apparatus mucosa, when people sucks too much, moreover it is possible to cause lung swelling, so that dead.Therefore the exploitation of the ammonia gas sensor of high sensitivity and low-detection lower limit is particularly important.It is known that electrochemical gas sensor, thermally conductive gas body sensor and semiconductor gas sensor are widely used this area.In the gas sensor of huge number, with conductor oxidate be sensitive material resistor-type gas sensor have highly sensitive, Monitoring lower-cut is low, selectivity good, response and the advantage such as resume speed is fast, all solid state, less costly, is one of current most widely used gas sensor.
The microstructure of sensitive material plays critically important effect at the aspect of performance improving gas sensor, and the method utilize silicon templated synthesis mesoporous material to improve material specific surface area, improving material gas-sensitive property is widely used.Material prepared by this hard template method is utilized to have the order network structure that degree of crystallinity is good.In addition, the surface of conductor oxidate supports noble metal receive significant attention to the method improving material air-sensitive performance, this method is possible not only to reduce the operating temperature of gas sensor, moreover it is possible to improve sensitivity and selectivity, gas sensitive modified in grow a lot potentiality.
WO3It is a kind of broad stopband n-type conductor oxidate, is widely used in NO owing to having outstanding sensitivity and selectivityx、O3And NH3Detection aspect.As n-type semiconductor oxide material, WO3Ammonia is had good sensitivity, adopts WO3As the research work of gas sensor of sensitive material by wide coverage the requirement having substantially met social application, but, improve sensitivity, reduce WO in the operating temperature of material3Also has very big research space.At present, based on mesoporous WO3Support the ammonia gas sensor of precious metals pt material and rarely have report, but noble metal can be good at improving the sensitivity of material and reducing the operating temperature of material, gas sensitive modified on application prospect good, therefore to mesoporous WO3The Research Significance of the ammonia gas sensor supporting precious metals pt material is far-reaching.
Summary of the invention
It is an object of the invention to provide a kind of based on the mesoporous WO supporting precious metals pt3The NH of material3Sensor and preparation method thereof.
Utilize the mesoporous WO supporting precious metals pt3Material is as sensitive material, and precious metals pt is at WO on the one hand3The surface of mesoporous material provides more reactivity site；Cubic structure KIT-6 template is utilized to be prepared for the WO with mesoporous shape characteristic on the other hand3Material, increases its specific surface area, and the combined effect of these two aspects is greatly improved the reaction efficiency of gas and sensitive material, and then improves the sensitivity of sensor.Meanwhile, commercially available tubular structure sensor manufacturing process of the present invention is simple, and volume is little, is beneficial to industrial batch production, therefore has important using value.
A kind of based on the mesoporous WO supporting precious metals pt3The NH of material3Gas sensor, by the outer surface Al with 2 discrete annular gold electrodes 42O3Insulating ceramics pipe 1, traverse Al2O3NI-G within insulating ceramics pipe 1 heats coil 3 and is coated in Al2O3Sensitive material film 2 on insulating ceramics pipe 1 outer surface and annular gold electrode 4 is constituted, and each annular gold electrode 4 is connected to a pair platinum filament 5, it is characterised in that: sensitive material film 2 is by the mesoporous WO supporting precious metals pt3Gained after material coating, the pore size of mesoporous material is 10～11nm, has regular meso-hole structure, and the degree of crystallinity of material is good, and precious metals pt major part is attached to inside mesopore orbit with simple substance form；The described mesoporous WO supporting precious metals pt3Material is prepared by following steps:
1. being dissolved in 10～30mL ethanol by the phosphotungstic acid of 0.5～1.0g, stirring is until being completely dissolved；Being dissolved in 10～30mL ethanol by the hard template mesopore molecular sieve KIT-6 of 0.4～0.7g, stirring is until being completely dissolved；
2. react 2～4 hours under 35 DEG C～55 DEG C water bath condition again after two kinds of solution mixing, until ethanol volatilizees completely；1～5h is sintered at 400～600 DEG C by dried at 60～80 DEG C for the pressed powder obtained；
3. being dissolved in 10～30mL ethanol by the phosphotungstic acid of 0.3～0.7g, stirring is until being completely dissolved；Whole sintered products step 2. obtained are dissolved in 10～30mL ethanol；React 2～4 hours under 35 DEG C～50 DEG C water bath condition again after two kinds of solution mixing, until ethanol volatilizees completely；1～3h is sintered at 400～600 DEG C by dried at 60～80 DEG C for the pressed powder obtained；
4. being dissolved in 10～30mL ethanol by the phosphotungstic acid of 0.05～0.25g, stirring is until being completely dissolved；Whole sintered products step 3. obtained are dissolved in 10～30mL ethanol；Again reacting 2～4 hours under 35 DEG C～50 DEG C water bath condition after two kinds of solution are mixed, until ethanol volatilizees completely；1～3h is sintered at 400～600 DEG C by dried at 60～80 DEG C for the pressed powder obtained；
5. the sintered product that 4. step obtains is dissolved in the hydrofluoric acid solution that concentration is 2～4mol/L, stir under room temperature 2～3 hours and KIT-6 template is removed, afterwards by the precipitate with deionized water generated and ethanol eccentric cleaning, dried sintering 1～2 hour under 400～450 DEG C of conditions again under 60～80 DEG C of conditions, thus obtaining the WO with meso-hole structure3Nano material powder；
The WO of the meso-hole structure 6. 5. step obtained3Nano material powder joins in ethanol, stirs and makes WO in 5～10 minutes3Nano material is uniformly dispersed, and is subsequently adding H2PtCl6Solution, stirs 5～10 minutes；H2PtCl6Consumption be WO30.5～1.0mol% of nano material；
7. mixed solution step 6. obtained reacts 2～4 hours under 35 DEG C～50 DEG C water bath condition, obtains supporting the WO of precious metals pt at 60～80 DEG C after drying3Mesoporous material powder.
Of the present invention a kind of based on the mesoporous WO supporting precious metals pt3The NH of material3The preparation method of gas sensor, its step is as follows:
1. the mesoporous WO of precious metals pt will be supported3Material powder mixes with deionized water 3～5:1 in mass ratio, and grinds formation pasty slurry, then takes a small amount of slurry and is uniformly coated on commercially available outer surface and carries the Al of 2 annular gold electrodes2O3Earthenware surface, forms the sensitive material film of 10～30 μ m-thick, and the length of earthenware is 4～4.5mm, and external diameter is 1.2～1.5mm, and internal diameter is 0.8～1.0mm, and makes sensitive material that annular gold electrode is completely covered；
2. toast 20～45 minutes under infrared lamp, treat that sensitive material is dried, Al2O3Earthenware sinters 2～3 hours at 400～450 DEG C；Then the NI-G that resistance value is 30～40 Ω is heated coil traverse Al2O3Above-mentioned device, as heater strip, finally is carried out welding and encapsulating by ceramic tube inside according to general heater-type gas sensor, thus obtaining based on the mesoporous WO supporting precious metals pt3The NH of material3Gas sensor.
Mesoporous WO prepared by the present invention3The gas sensor supporting precious metals pt material has the advantage that
1. utilizing immersion method to prepare this sensitive material, synthetic method is simple, with low cost；
2. utilize hard template method to prepare mesoporous WO3, preparation method is simple, has stable meso-hole structure, and material crystalline degree is good, effectively raises the specific surface area of material；
3. by WO3Upper dipping H2PtCl6Solution, successfully makes noble metal be supported on mesoporous WO3On, the combination of bi-material, improve NH3Sensitivity, reduce the optimum working temperature of material and there is good reversibility, detection NH3Content aspect has broad application prospects；
4. adopting commercially available tubular type sensor, device technology is simple, and volume is little, is suitable to produce in enormous quantities.
Accompanying drawing explanation
Fig. 1: support the mesoporous WO of precious metals pt3The TEM shape appearance figure of material, wherein the amplification of illustration is 50000 times；
Fig. 2: support the mesoporous WO of precious metals pt3The little angle figure of XRD of material；
Fig. 3: support the mesoporous WO of precious metals pt3The XRD Radix Rumicis figure of material；
Fig. 4: support the mesoporous WO of precious metals pt3The NH of material3The structural representation of sensor；
Fig. 5: comparative example and in embodiment at sensor different operating temperature, NH3Concentration is the Sensitivity comparison figure under 200ppm；
Fig. 6: comparative example and sensor NH to variable concentrations under optimum working temperature in embodiment3Sensitivity comparison figure；
As it is shown in figure 1, figure can be seen that WO3For ordered structure, pore size is 10～11nm；
As in figure 2 it is shown, figure supports the mesoporous WO of Pt3Mesoporous WO with undoped p Pt3Go out peak position identical, go out peak at (211) place sharp-pointed, illustrate that both materials have long-range order；
As it is shown on figure 3, XRD spectra represents the mesoporous WO supporting Pt3With WO3Base peak is completely corresponding；
As shown in Figure 4, device is by Al2O3Earthenware 1, quasiconductor sensitive material 2, nickel-cadmium coil 3, annular gold electrode 4 and platinum line 5 form；
As it is shown in figure 5, when device is at NH3Gas concentration is under 200ppm, and the optimum working temperature of comparative example and embodiment respectively 200 DEG C and 125 DEG C, now device is to 200ppmNH3Sensitivity respectively 7.1 and 13.6；
As shown in Figure 6, when device under respective optimum working temperature, the sensitivity of device is along with NH3The increase of concentration and increase, embodiment is to 50～1500ppmNH3Sensitivity be 6.7～23.4, and comparative example is to 50～1500ppmNH3Sensitivity be only 2.6～12.2, wherein, sensitivity is sensor resistance value R in gas to be measuredgWith aerial resistance value RaRatio, be expressed as: S=Rg/Ra。
Detailed description of the invention
Comparative example 1:
With mesoporous WO3Material makes heater-type NH as sensitive material3Sensor, its concrete manufacturing process:
1. first take 0.7g phosphotungstic acid and 0.5gKIT-6 is dissolved in 20mL ethanol respectively, two kinds of solution mixing are placed under 50 DEG C of water bath condition and react 4 hours, dried by powder high temperature sintering 4 hours under 500 DEG C of conditions at 70 DEG C；In order to improve the filling to KIT-6 duct, then being repeated twice by aforesaid operations, be namely joined by the alcoholic solution of whole sintered products just prepared in the alcoholic solution of phosphotungstic acid, the consumption of phosphotungstic acid is reduced to 0.35g and 0.15g successively, and all the other conditions are constant；The product that final compound obtains is sintered 2h at 600 DEG C.
2. the powder of about 1.7g after above-mentioned sintering is dissolved in the 40mL hydrofluoric acid solution that concentration is 4mol/L, stir under room temperature 2 hours and KIT-6 template is removed, afterwards by the precipitate with deionized water generated and ethanol repeatedly eccentric cleaning, 70 DEG C of dried sintering 2 hours at 450 DEG C again, thus obtaining the WO with meso-hole structure3Nano material 1.2g.The specific surface area of resulting materials is 77.45m2/g。
3. taking a small amount of prepared sensitive material powder, 5:1 instills deionized water in mass ratio, grinds to form pasty slurry.Then dip a small amount of slurry with brush to be uniformly coated on commercially available outer surface and carry the Al of 2 annular gold electrodes2O3Earthenware surface, forms the sensitive material film of 30 μ m-thick, and the length of earthenware is 4mm, and external diameter is 1.2mm, and internal diameter is 0.8mm, and makes sensitive material that annular gold electrode is completely covered；
4. toast 30 minutes under infrared lamp, treat that sensitive material is dried, Al2O3Earthenware sinters 2 hours at 400 DEG C；Then the nickel-cadmium coil that resistance value is 30 Ω is passed Al2O3Above-mentioned device, as heater strip, finally is carried out welding and encapsulating by ceramic tube inside according to general heater-type gas sensor, thus obtaining mesoporous WO3Material makes heater-type NH as sensitive material3Sensor.
Embodiment 1:
With the mesoporous WO supporting precious metals pt3Material makes NH as sensitive material3Sensor, its concrete manufacturing process:
1. first take 0.7g phosphotungstic acid and 0.5gKIT-6 is dissolved in 20mL ethanol respectively, two kinds of solution mixing are placed under 50 DEG C of water bath condition and react 4 hours, dried by powder high temperature sintering 3 hours under 500 DEG C of conditions at 70 DEG C；In order to improve the filling to KIT-6 duct, then being repeated twice by aforesaid operations, be namely joined by the alcoholic solution of whole sintered products just prepared in the alcoholic solution of phosphotungstic acid, the consumption of phosphotungstic acid is reduced to 0.35g and 0.15g successively, and all the other conditions are constant；The product that final compound obtains is sintered 2h at 600 DEG C.
2. the powder of about 1.7g after above-mentioned sintering is dissolved in the 40mL hydrofluoric acid solution that concentration is 4mol/L, stir under room temperature 2 hours and KIT-6 template is removed, afterwards by the precipitate with deionized water generated and ethanol repeatedly eccentric cleaning, 70 DEG C of dried sintering 2 hours at 450 DEG C again, thus obtaining the WO with meso-hole structure3Nano material 1.2g.
3. take above-mentioned mesoporous WO3The powder of material joins in 20mL alcoholic solution, stirs and makes mesoporous WO in 10 minutes3Powder is thoroughly dispersed in alcoholic solution, is subsequently adding WO3The H of the 0.5mol% of powder2PtCl6Solution, stirs 10 minutes；
4. being placed in the water-bath of 45 DEG C by above-mentioned mixing liquid, react 2 hours, 70 DEG C of powder obtained after drying are the mesoporous WO supporting precious metals pt3Material, the specific surface area of resulting materials is 82.05m2/g。
5. the mesoporous WO that will obtain3The powder supporting precious metals pt material mixes with deionized water 5:1 in mass ratio, and grinds formation pasty slurry, then dips a small amount of slurry with brush and is uniformly coated on commercially available outer surface and carries the Al of 2 annular gold electrodes2O3Earthenware surface, forms the sensitive material film of 30 μ m-thick, and the length of earthenware is 4mm, and external diameter is 1.2mm, and internal diameter is 0.8mm, and makes sensitive material that annular gold electrode is completely covered；
6. toast 30 minutes under infrared lamp, treat that sensitive material is dried, Al2O3Earthenware sinters 2 hours at 400 DEG C；Then the nickel-cadmium coil that resistance value is 30 Ω is passed Al2O3Above-mentioned device, as heater strip, finally is carried out welding and encapsulating by ceramic tube inside according to general heater-type gas sensor, thus obtaining mesoporous WO3Support the precious metals pt material NH as sensitive material3Sensor.
Claims (4)
1. one kind based on the mesoporous WO supporting precious metals pt3The NH of material3Gas sensor, by the outer surface Al with 2 discrete annular gold electrodes 42O3Insulating ceramics pipe (1), traverse Al2O3The NI-G of insulating ceramics pipe (1) inside heats coil (3) and is coated in Al2O3Sensitive material film (2) on insulating ceramics pipe (1) outer surface and annular gold electrode (4) is constituted, each annular gold electrode (4) is connected to a pair platinum filament (5), it is characterised in that: sensitive material film (2) is by the mesoporous WO supporting precious metals pt3Gained after material coating, the pore size of mesoporous material is 10～11nm, has regular meso-hole structure, and the degree of crystallinity of material is good, and precious metals pt major part is attached to inside mesopore orbit with simple substance form；The described mesoporous WO supporting precious metals pt3Material is prepared by following steps:
1. being dissolved in 10～30mL ethanol by the phosphotungstic acid of 0.5～1.0g, stirring is until being completely dissolved；Being dissolved in 10～30mL ethanol by the hard template mesopore molecular sieve KIT-6 of 0.4～0.7g, stirring is until being completely dissolved；
2. react 2～4 hours under 35 DEG C～55 DEG C water bath condition again after two kinds of solution mixing, until ethanol volatilizees completely；1～5h is sintered at 400～600 DEG C by dried at 60～80 DEG C for the pressed powder obtained；
3. being dissolved in 10～30mL ethanol by the phosphotungstic acid of 0.3～0.7g, stirring is until being completely dissolved；Whole sintered products step 2. obtained are dissolved in 10～30mL ethanol；React 2～4 hours under 35 DEG C～50 DEG C water bath condition again after two kinds of solution mixing, until ethanol volatilizees completely；1～3h is sintered at 400～600 DEG C by dried at 60～80 DEG C for the pressed powder obtained；
4. being dissolved in 10～30mL ethanol by the phosphotungstic acid of 0.05～0.25g, stirring is until being completely dissolved；Whole sintered products step 3. obtained are dissolved in 10～30mL ethanol；Again reacting 2～4 hours under 35 DEG C～50 DEG C water bath condition after two kinds of solution are mixed, until ethanol volatilizees completely；1～3h is sintered at 400～600 DEG C by dried at 60～80 DEG C for the pressed powder obtained；
5. the sintered product that 4. step obtains is dissolved in the hydrofluoric acid solution that concentration is 2～4mol/L, stir under room temperature 2～3 hours and KIT-6 template is removed, afterwards by the precipitate with deionized water generated and ethanol eccentric cleaning, dried sintering 1～2 hour under 400～450 DEG C of conditions again under 60～80 DEG C of conditions, thus obtaining the WO with meso-hole structure3Nano material powder；
The WO of the meso-hole structure 6. 5. step obtained3Nano material powder joins in ethanol, stirs and makes WO in 5～10 minutes3Nano material is uniformly dispersed, and is subsequently adding H2PtCl6Solution, stirs 5～10 minutes；H2PtCl6Consumption be WO30.5～1.0mol% of nano material；
7. mixed solution step 6. obtained reacts 2～4 hours under 35 DEG C～50 DEG C water bath condition, obtains supporting the WO of precious metals pt at 60～80 DEG C after drying3Mesoporous material powder.
2. a kind of based on the mesoporous WO supporting precious metals pt as claimed in claim 13The NH of material3Gas sensor, it is characterised in that: the thickness of sensitive material film (2) is 10～30 μm.
3. a kind of based on the mesoporous WO supporting precious metals pt as claimed in claim 13The NH of material3Gas sensor, it is characterised in that: Al2O3The length of insulating ceramics pipe (1) is 4～4.5mm, and external diameter is 1.2～1.5mm, and internal diameter is 0.8～1.0mm.
4. a kind of based on the mesoporous WO supporting precious metals pt described in claim 13The NH of material3The preparation method of gas sensor, its step is as follows:
1. the mesoporous WO of precious metals pt will be supported3Material powder mixes with deionized water 3～5:1 in mass ratio, and grinds formation pasty slurry, then takes a small amount of slurry and is uniformly coated on commercially available outer surface and carries the Al of 2 annular gold electrodes2O3Earthenware surface, forms the sensitive material film of 10～30 μ m-thick and makes sensitive material that annular gold electrode is completely covered；
2. toast 20～45 minutes under infrared lamp, treat that sensitive material is dried, Al2O3Earthenware sinters 2～3 hours at 400～450 DEG C；Then the NI-G that resistance value is 30～40 Ω is heated coil traverse Al2O3Above-mentioned device, as heater strip, finally is carried out welding and encapsulating by ceramic tube inside according to general heater-type gas sensor, thus obtaining based on the mesoporous WO supporting precious metals pt3The NH of material3Gas sensor.
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| CN106365204A (en) * | 2016-11-03 | 2017-02-01 | 河北工业大学 | Preparation method of tungsten trioxide sensitive material for ammonia gas sensitive sensor |
| CN107064235A (en) * | 2016-11-02 | 2017-08-18 | 景德镇学院 | A kind of Pt nanoparticles modify ZnSnO3The preparation method of nanosheet gas-sensitive material |
| CN109490371A (en) * | 2018-11-28 | 2019-03-19 | 中国华能集团有限公司 | A kind of methylamine monitor and preparation method thereof |
| CN109781796A (en) * | 2019-03-06 | 2019-05-21 | 东北大学 | A kind of NO preparing ZnS-ZnO hetero-junctions nano particle based on zincblende2Gas sensor |
| CN110426420A (en) * | 2019-08-08 | 2019-11-08 | 东北大学 | One kind WO as made of nanometer rods self assembly3The NH of micron shuttle3Gas sensor and preparation method thereof |
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| CN113406155A (en) * | 2021-06-23 | 2021-09-17 | 长春理工大学 | Tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and preparation method thereof |
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| CN109490371A (en) * | 2018-11-28 | 2019-03-19 | 中国华能集团有限公司 | A kind of methylamine monitor and preparation method thereof |
| CN109781796A (en) * | 2019-03-06 | 2019-05-21 | 东北大学 | A kind of NO preparing ZnS-ZnO hetero-junctions nano particle based on zincblende2Gas sensor |
| CN110426420A (en) * | 2019-08-08 | 2019-11-08 | 东北大学 | One kind WO as made of nanometer rods self assembly3The NH of micron shuttle3Gas sensor and preparation method thereof |
| CN110879238A (en) * | 2019-10-25 | 2020-03-13 | 东北大学 | Molybdenum trioxide nano-structure sensitive material, corresponding ammonia gas sensor and preparation method |
| CN110879238B (en) * | 2019-10-25 | 2021-08-24 | 东北大学 | Molybdenum trioxide nano-structure sensitive material, corresponding ammonia gas sensor and preparation method |
| CN113406155A (en) * | 2021-06-23 | 2021-09-17 | 长春理工大学 | Tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and preparation method thereof |
| CN113758974A (en) * | 2021-08-30 | 2021-12-07 | 中国科学院合肥物质科学研究院 | Oxide semiconductor gas sensor and preparation method and application thereof |
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